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Considerations for nanomaterial identification of powders using volume-specific surface area method
(2019)
The EC’s recommendation for a definition of nanomaterial (2011/696/EU) should allow the identification of a particulate nanomaterial based on the number-based metric criterion according to which at least 50% of the constituent particles have the smallest dimension between 1 and 100 nm. However, it has been recently demonstrated that the implementation of this definition for regulatory purposes is conditioned by the large deviations between the results obtained by different sizing methods or due to practical reasons such as high costs and time-consuming.
For most measurement methods for particle size determination it is necessary to initially disperse the particles in a suitable liquid. However, as the particle size decreases, the adhesion forces increase strongly, making it more difficult to deagglomerate the particles and to assess accurately the result of this process. Therefore, the success of the deagglomeration process substantially determines the measurement uncertainty and hence, the comparability between different methods.
Many common methods such as dynamic light scattering (DLS), centrifugal liquid sedimentation (CLS) or ultrasound attenuation spectroscopy (US) can give good comparable results for the size of nanoparticles, if they are properly separated and stabilized (e.g. in reference suspensions).
In order to avoid the use of hardly available and expensive methods such as SEM / TEM for all powders, an agglomeration-tolerant screening method is useful.
One of the measurement methods well suited to probe the size of particulate powder is the determination of the volume-specific surface area (VSSA) by means of gas adsorption as well as skeletal density. The value of 60 m2/cm3 corresponding to spherical, monodisperse particles with a diameter of 100 nm constitutes the threshold for decisioning if the material is a nano- or non-nanomaterial. The identification of a nanomaterial by VSSA method is accepted by the EU recommendation.
However, the application of the VSSA method was associated also with some limitations. The threshold of 60 m2/cm3 is dependent on the particle shape, so that it changes considerably with the number of nano-dimensions, but also with the degree of sphericity of the particles. For particles containing micro-pores or having a microporous coating, false positive results are induced. Furthermore, broad particle size distributions made necessary to additionally correct the threshold. Based on examples of commercially available ceramic powders, the applicability of the VSSA approach was tested in relation with SEM and TEM measurements. The introduction of a correction term for deviations from sphericity and further additions improved the applicability of VSSA as a screening method.
Nominal-actual comparisons are routinely performed to compare a manufactured specimen to a reference specimen. X-ray Computed Tomography (CT) has brought a profound change in the way that tolerance verifications are performed in industry, by allowing the inner and outer geometries of an object to be measured, without the need for external access or destructive testing. As a results, CT is increasingly used in additive manufacturing applications, where a nominal-actual comparison performed between the digital model (CAD file), used as an input for the 3D printer, and the CT volume from the printed part, can provide invaluable information as to the accuracy of the printing process. However, the nominal-actual comparison process is somewhat different when applied to additively manufactured specimens by comparison to conventionally manufactured specimens.
Polymeric membranes represent a low-cost, energy efficient solution for gas separation. Recently polymers of intrinsic microporosity (PIMs) have emerged as prestigious membrane materials featuring a large concentration of pores smaller than 1 nm, a BET surface area larger than 700 m2/g and high gas permeability and selectivity. Unusual chain structure combining rigid segments with sites of contortion gives rise to the intrinsic microporosity. However, this novel class of glassy polymers are prone to pronounced physical aging. The initial microporous structures approach a denser state via local small scale fluctuataions, leading to a dramatic reduction in the gas permeabilities. For the first time, dielectric relaxation spectroscopy with state-of-the-art high-resolution analyzers was employed to investigate three representative PIMs with a systematic change in chain rigidity: PIM-EA-TB 〉 PIM-1 〉 PIM-MDPH-TB. The molecular mobility, the charge transport and their response upon heating (aging) in the polymers were measured in a broad temperature range through isothermal frequency scans during different heating / cooling cycles. Multiple dielectric processes following Arrhenius behavior were observed for the investigated polymers. Local fluctuations, Maxwell-Wagner-Sillars (MWS) polarization and structural relaxation phenomena were discussed and attempted to be correlated with the structural features of PIMs. Moreover, all PIMs showed conductivity in the glassy state. The significant increase in the conductivity with increasing temperature far below the glass transition temperature of PIMs is explained in terms of the loosely packed microporous structure and the formation of local intermolecular agglomerates due to interaction of π-electrons in aromatic moieties of the polymer backbone.
New Focus On Boehmite-Reinforced Nanocomposites Molecular Approach With Advanced FTIR-Techniques
(2019)
By FTIR-study it was possible to proof a chemical reaction between boehmite and the hardener of anhydride cured epoxy resins. Future studies can assume that the chemical environment of the resin system is changed in the surrounding of boehmite nanoparticles. This highly affects especially localized properties.
Evolution of a friction material with braking sequence: properties related to the microstructure
(2019)
The microstructural complexity (multi-component and multi-scale) of friction materials, such as those used in braking applications,usually limits the characterization to the pristine state, even when they are to be submitted to high loading brake sequences. The understanding of properties ageing as a function of load history and microstructure is an important step to gain further knowledge on the tribological mechanisms occurring at the contact surface, as well as on the braking performances. To do so, the bulk mechanical and microscopical properties of a semi-metallic friction material are investigated before and after a braking sequence. Uniaxial compression tests combined with DIC are used to study the axial evolution of the mechanical behaviour (i.e., from the contact surface to the backplate). A significant mechanical evolution is observed in the after-braking material, which develops a layered behaviour along the depth. The layers (three) exhibit distinct mechanical/microstructural features that can be related to the braking thermal gradients and the occurrence of local damage.
In this work, the structural integrity of LBM fabricated IN625 small cylinders (d = 1 mm, h = 6 mm) was investigated regarding the porosity and the surface roughness by means of computed tomography. The measurements were carried out on a GE v|tome|x L 300/180 with a reconstructed voxel size of 2 µm. The pores were analyzed for size, shape and spatial distribution. The correlation between compactness C and spatial distribution showed that elongated pores (C < 0.2) appear exclusively within a distance of 80 µm to the sample surface. The reconstructed surface was digitally meshed and unwrapped to evaluate the mean roughness Ra. Since the gravity correlates linearly with the sine of the build angle, the influence of gravity on porosity and surface roughness was determined.
Nanocomposites are extremely versatile due to their physicochemical properties, which differ significantly from bulk homopolymers. One of the inorganic nanomaterials which are increasingly used as a filler in polymer matrices is boehmite, typically used as an inexpensive flame retardant. Here, it is used as a nanofiller in polycarbonate and polyamide, expecting to improve their mechanical properties. For industrial use boehmite is obtained by the solvothermal method, resulting in a layered nanomaterial, whereas naturally it occurs as single crystals with the size of <100µm. In this work we are obtaining and isolating boehmite crystals by a bottom-up method, in which a reaction between aluminum nitride and sodium hydroxide. Obtaining boehmite as microcrystals is necessary for its analysis and characterization, as well as to investigate its interaction with polymer matrices at the polymer/particle interface. Here, the obtained particles in polymer matrices are characterized with differential scanning calorimetry and thermogravimetry analysis.
Nanocomposites are extremely versatile due to their physicochemical properties, which differ significantly from bulk homopolymers. One of the inorganic nanomaterials which are increasingly used as a filler in polymer matrices is boehmite, typically used as an inexpensive flame retardant. Here, it is used as a nanofiller in polycarbonate and polyamide, expecting to improve their mechanical properties. For industrial use boehmite is obtained by the solvothermal method, resulting in a layered nanomaterial, whereas naturally it occurs as single crystals with the size of <100µm. In this work we are obtaining and isolating boehmite crystals by a bottom-up method, in which a reaction between aluminum nitride and sodium hydroxide. Obtaining boehmite as microcrystals is necessary for its analysis and characterization, as well as to investigate its interaction with polymer matrices at the polymer/particle interface. Here, the obtained particles in polymer matrices are characterized with differential scanning calorimetry and thermogravimetry analysis.
In well-annealed thin polymer films, with non-repulsive polymer/substrate interactions, an irreversibly adsorbed layer is formed. These adsorbed layers have shown enormous potential for technological applications. The growth kinetics and molecular dynamics of these buried layers in thin films are still not fully investigated due to the hard accessibility. Here, the irreversibly adsorbed layers of homopolymer thin films are revealed by solvent-leaching experiments. The growth kinetics of these layers is investigated as a function of original film thickness and annealing times. The thickness, topography and quality of the adsorbed layer is determined with Atomic Force Microscopy (AFM) and spectroscopic ellipsometry. Additionally, the molecular mobility of the adsorbed layer is investigated with Broadband Dielectric Spectroscopy (BDS). A recently developed nanostructured capacitor (NSC) is employed to measure the adsorbed layers with a free surface layer depending on annealing and solvent-leaching time. The results are quantitatively compared and discussed with respect to recently published work.
Over the past decades research on the molecular dynamics of miscible polymer blends is of topical interest in the literature, to understand the segmental mobility of individual components, as it is affected by blending. In general, miscible polymer blends exhibit a complex dynamic behavior. For an A/B blend the relaxation times of component A and component B are affected by the spatial local compositional heterogeneity, present in binary systems on a microscopic level, regardless of the macroscopic homogeneity. Here, a combination of broadband dielectric and specific heat spectroscopy was employed to study the dynamically asymmetric PVME/PS blend with seven different compositions, focusing on samples with high PS contents. Considering that PS is dielectrically invisible, BDS is a powerful technique to study the response of PVME, as it is affected by PS segments. Here, three separate relaxation processes were found by dielectric investigations, related to confined or constrained PVME segments due to the spatial local compositional heterogeneities, which is in contrary to the previous literature findings [1]. Moreover, the dielectric data was compared with results obtained by specific heat spectroscopy, where a fourth relaxation process was found, due to the cooperative fluctuations of PVME and PS.
[1] Colmenero, J., Arbe, A. Soft Matter, 2007, 3, 1474.
Mechanochemistry paves the way to simple, fast, and green syntheses. Despite considerable effort, there remains a lack in understanding of the underlying mechanisms. In situ investigations help to understand these mechanisms, which occur during a mechanochemical reaction. Here we present a universal strategy for simultaneous real-time in situ analysis, combining X-ray diffraction, Raman spectroscopy, and thermography. The potential of our approach is shown for different model reactions.
Fresh cement paste is a suspension consisting of a hydraulic binder (cement), water, and numerous minor components – admixtures. Addition of admixtures aims at specific modification of properties of the fresh cement paste or hardened cementitious building material. Specific admixtures, so-called superplasticizers (SP), are used to improve the flowability of the fresh cement paste with reduced water content. The latter is the starting material for the high-strength concrete. Thus, SPs are essential for the ambitious construction projects.
However, uncontrollable retardation of the setting time in presence of SPs is occasionally observed. Obviously, SPs influence early products of the cement hydration leading to changes in the microstructure development. The hardening is thus delayed, and the quality of the resulting building material suffers. The mechanisms of the admixture action during the hydration process are still intensively investigated [1-7]. A detailed understanding of the admixture effects during the early hydration stage is the key to control and individual adjustment of the cement-based construction materials.
We use the unique combination of the wall-free sample holder and the time-resolved X-ray scattering analysis to achieve the full information about the hydrate phases formed under the influence of admixtures. We use ultrasonic levitator to start the cement hydration in levitated cement pellets [8, 9]. The sample levitation allows collection of the unimpaired information about cement hydrate phases. The most beneficial is the avoiding of the contributions of the sample holder material to the data signal.
We induce the cement hydration by adding water to unhydrated Portland cement during the data acquisition. The full phase composition of the hydrating cementitious system can be gathered in situ using wide angle X-ray scattering (WAXS). During the hydration of cement both crystalline and amorphous hydrate phases are formed. WAXS data contain the information about crystalline phases behind the Bragg reflections, whereas the amorphous hydrates influence the appearance of the background. Application of the data analysis specific for crystalline or amorphous phases is needed. The data quantification by the Rietveld method allows to conclude about the changes of the phase amounts due to the presence of admixture. The calculation of the pair distribution functions allows analysis of the amorphous hydrates. Based on this information, the SP effects and the extent of their involvement into the ongoing reactions can be concluded. A detailed understanding of the complex cement hydration process is envisioned.
Ziel des Projektes HARFE (Haftfestigkeit Reproduzierbarkeit Festigkeit) war es, eine Er-höhung der Haft- bzw. Klebfestigkeit auf Niedrigenergie-Polymeren (PE, PP, PTFE) zu erreichen. SENTECH realisierte dazu plasmachemische Oberflächenaktivierungen mit O2 und die Abscheidung von Aluminiumoxidschichten (Al2O3) mittels Atomic Layer Deposition (ALD), wobei die Ellipsometrie zum in-situ Monitoring der ALD-Prozesse diente. Die BAM charakterisierte die modifizierten Oberflächen bezüglich der Oberflächenenergie (OFE) und bestimmte die Verbund- bzw. Klebfestigkeit mittels der Zentrifugentechnologie
Coating materials are nowadays often required to deliver not only sufficient barrier performance and suited optical appearance but a broad range of other functional properties. The incorporation of inorganic nanoparticles (NPs) is known to improve many key characteristics and provide new functionalities in polymer materials. Presented work aims to prepare and characterize an organic-inorganic coating material designed to bring together advantageous properties of hybrid materials and reinforcement effect delivered from the inorganic NPs embedment.
Siloxane-based hybrid resins hold great advantages as coating materials as their properties can be tuned between those of polymers and those of glasses, thus, the compositions with superior thermal and mechanical properties can be achieved. We used Cycloaliphatic Epoxy Oligosiloxane (CEOS) resin as a polymeric matrix where the network formation was achieved by UV induced cationic polymerisation. Boehmite Alumina (BA) nanoparticles were added to CEOS resin as a reinforcing agent and resultant material was processed into films either by bar-coating or by spin-coating depending on further characterization procedure. Two different types of BA NPs, hydrophilic and organophilic, were used in order to assess the impact of particles surface on the resin characteristics. CEOS synthesis by condensation reaction was confirmed using 13C and 29Si NMR. Changes in CEOS photocuring process, resulting from particles incorporation, were monitored by real-time IR spectroscopy. At the same time, the thermal behaviour was evaluated by DSC and TGA methods. Morphology of the coatings was investigated by means of SEM operated in transmission mode.
It was observed that BA presence increased the epoxy conversion degree and glass transition temperature. Material formulations providing best film characteristics were determined with regard to the particle type and loading. Compared to the hydrophilic nanoparticles, organophilic BA NPs yield superior overall performance of the foils.
Since the early 19th century microorganisms were studied on their capabilities of causing microbiologically influenced corrosion (MIC) of metals. The most studied ones are sulfate-reducing bacteria (SRB), but others can corrode metals as well, e.g. acid-producing bacteria or methanogenic archaea (MA). However, these studies were mostly focused on metals related to the petroleum industry but metals for other industries, e.g. dentistry, are also susceptible to corrosion. The inert Titanium (Ti) is often used as an implant material, but it is a base metal. The formation of a passivating oxide layer allows Ti to be corrosion resistant at normal conditions.
Nonetheless, scanning electron microscope images on dental implants from patients with acute peri-implantitis showed clear signs of corrosion. Currently, the corrosion mechanism of dental implants is unknown, but many indications suggest that oral microorganisms, including MA (Methanobrevibacter oralis) and SRB (Desulfomicrobium orale), could be involved.
To determine if MA or SRB can corrode Ti (pure Ti or Ti-6Al-4V alloy), corrosion rate, methane and sulfide concentrations were analyzed. Electrical potential measurements using in-house developed electrochemical cells indicated a potential change on Ti in the presence of a corrosive MA strain compared to an abiotic control.
Microbial composition comparison will be analyzed using samples from dental pockets of 150 infected patients by considering the quality of the implant and 50 healthy people by means of amplicon sequencing. Enrichments and isolation of pure cultures from the dentals samples are also examined for their corrosion behavior. Overall, this is the first study investigating the susceptibility of dental implant material to corrosion using human related MA.
Up to now, the mechanisms of surface nucleation and surface-induced texture formation are far from being understood. Very few observations of crystal orientation were focused on separately growing surface crystals. In conclusion, no systematic studies on initially oriented crystal growth or nucleation from defined active surface nucleation sites exists. Therefore, the main objective of this just is to advance the basic understanding of the mechanisms of surface-induced microstructure formation in glass ceramics. As a first attempt, we focus on reorientation of separately growing surface crystals during their early growth.
Polymeric core-shell particles were synthesized in a semi-batch emulsion polymerization process. The shell of the particles consist of PVDF with a high amount of beta-phase. Small-angle X-ray scattering (SAXS) was used to quantify the size of the cores of the particles and the thickness of the shell.
Absorption edge tomography is a method which exploits the sudden change of the attenuation coefficient, when the photon energy crosses the absorption edge of an element. The beamline BAM line at BESSY II, which is operated by the Federal Institute for Materials Research and Testing, can provide a monochromatized beam in a photon energy range from 5 keV up to 80 keV with a bandwidth of 2%. Together with the microtomography setup, this enables differential tomography sensitive to any element with N >= 24 (Cr) by using an appropriate K- or L-edge in this range. Here, a polymer filament embedding metal organic framework (MOF) was prepared and used for 3D printing. Absorption edge tomography at the copper K edge was employed to perform a non-destructive 3D characterization of the microstructure of the embedded MOF. Data fusion was then used to determine the size distribution of the embedded MOF.
Fiber reinforced polymers (FRPs) are a well established material in lightweight applications, e.g. in automotive, aerospace or wind energy. The FRP components are subjected to multiaxial mechanical as well as hygrothermal loads. Common operation temperatures are in the range of 213 K and 373 K (-60 °C and 100 °C) at a relative humidity of 10% to 90%. In spacecraft applications, the environmental conditions are even more extreme. However, the correlation between multiaxial mechanical loading and harsh environment conditions have to-date not been investigated in detail. The project aims to investigate the fatigue behavior of FRPs dependent on multiaxial mechanical loading, temperature, and humidity. Extensive experimental testing is performed on flat plate and cylindrical tube specimens, accompanied by numerical and analytical calculations.
Using non-optimum combination of manufacturing parameters in selective laser melting (SLM) may lead to reduction of quality of component: defects generation, distortion of geometry and even cracking. Usually, the optimization of parameters is performed by changing volumetric energy density (Ev) and selecting parameters giving low porosity values. However, not only low porosity but also stable microstructure and low residual stresses will help to achieve advanced mechanical behavior of the component.
In present work, we investigated cuboid-shaped Ti-6Al-4V samples produced with different manufacturing parameters. The parameters leading to the same Ev were considered as well as parameters which are not included in Ev. Residual stresses in subsurface region were investigated by synchrotron X-ray diffraction, which allows to penetrate around 100 µm from the surface therefore overcome the problem of high roughness of SLM components without additional sample preparation. Only tensile stresses were found along the building direction, that can play critical role especially during cyclic loading. In parallel, using X-ray computed tomography we also observe that porosity is mainly concentrated in the contour region, except in case where the laser speed is small. However, by using some process parameters it was possible to decrease residual stresses and obtain uniform α+β Ti microstructure and relatively low porosity. Additionally, it was found that not included in Ev (e.g., base plate position, focus distance) should be considered as additional manufacturing parameters during SLM process.
The porosity and the surface roughness are recently discussed problems for SLM parts. The influence of SLM process parameters on porosity is well studied for different materials. Nevertheless, the build angle (i.e. the angle between part orientation and build plate) needs to be understood as an additional SLM process parameter, as it has been shown, that the microstructure and hence the mechanical performance of various materials depend on the build angle. The inherent build angle of each strut as a part of a lattice structure is the motivation to investigate the influence of the build angle on the porosity and roughness on round-shaped (1 mm diameter) struts by means of CT. Conventional Coordinate Measuring Machine (CMM) has the limitation towards small and round shaped samples. The need for Computed Tomography (CT) regarding investigations of SLM parts will increase because no other non-destructive technique allows the assessment of complex geometries with inner laying surfaces. We used CT to assess the pores and the strut surface. Seven struts out of the nickel alloy Inconel 625 with build angles from 30° to 90° were studied. It was found that the number of pores is smaller, and the size of pores is larger for the 90° strut. In case of 30° strut, the number of pores is increased towards down-skin side, additionally, this strut orientation showed to have the largest number of attached powder particles. The elongated pores exist exclusively near the strut surface. While the roughness at the down-skin surface is highly depending of the biud angle, the roughness at the up-skin surface is the same for all struts. The mechanisms of pore and surface roughness formation is not mainly driven by gravity.
Additive manufacturing (AM) opens the route to a range of novel applications. However, the complexity of the manufacturing process poses a challenge to produce defect-free parts with a high reliability. Since process dynamics and resulting microstructures of AM parts are strongly influenced by the involved temperature fields and cooling rates, thermography is a valuable tool for process monitoring. Another approach to monitor the energy input into the part during process is the use of optical tomography.
Common visual camera systems reach much higher spatial resolution than infrared thermography cameras, whereas infrared thermography provides a much higher temperature dynamic. Therefore, the combined application increases the depth of information. Here, we present first measurement results using a laser beam melting setup that allows simultaneous acquisition of thermography and optical tomography from the same point of view using a beam splitter. A high-resolution CMOS camera operating in the visible spectral range is equipped with a near infrared bandpass filter and images of the build plate are recorded with long-term exposure during the whole layer exposing time. Thus, areas that reach higher maximum temperature or are at elevated temperature for an extended period of time appear brighter in the images. The used thermography camera is sensitive to the mid wavelength infrared range and records thermal videos of each layer exposure at an acquisition rate close to 1 kHz.
As a next step, we will use computer tomographic data of the built part as a reference for defect detection.
This research was funded by BAM within the focus area Materials.
An increase in the thermal diffusivity of Fe2TiO5 is observed after only three cycles of measurement. X-ray refraction shows an increase in the mean specific surface. A segregation of Ca- and F-rich nanocrystals at grain boundaries is also observed by SEM and STEM-EDX. This emphasizes the importance of precursor purity and the influence of redistribution of impurities on thermoelectric properties.
Additive Manufacturing (AM) offers the opportunity to produce easier geometrically complex parts compared to traditional production technologies. An important AM technology for metals is selective laser melting (SLM) where a part is produced by melting and solidifying powder in layers. This technique is known to cause a pronounced texture in the produced AM products due to the specific heat flow and the associated solidification of the material during SLM deposition. In order to evaluate the influence of the deposition hatch length during SLM of nickel based superalloy Inconel 718 samples on the texture and in order to identify any preferred crystallographic direction, we performed monochromatic neutron radiography scans (using wavelength from 1.6 Å to 4.4 Å, step size 0.05 Å) to image the samples while rotating it through 90°. Samples produced with short hatch length showed fine textured columnar grains oriented along the sample building direction in high-resolution radiographs. Whereas processing the sample using a ten-fold longer hatch length reduced the texture. The neutron radiographic experiments were accompanied by scanning electron microscopy including electron back-scattered diffraction to visualize and verify the microstructure and texture.
Additive Manufacturing by Selective Laser Melting (SLM) offers an ample scope for producing geometrically complex parts as compared to the traditional subtractive manufacturing strategies. However, the residual stresses (RS) developed during the processing can reduce the load bearing capacity as well as induce unwanted distortion, limiting the life time and the application of SLM parts.
Due to the advantages of additive manufacturing (AM), it has been increasingly integrated into many industrial sectors.
The application of AM materials for safety-critical parts requires the detailed knowledge about their microstructure stability under thermo-mechanical or mechanical load and knowledge on ageing process mechanisms. Ageing processes are characterized by change of the material microstructure that is to be initially investigated. This work deals with the Investigation of 316L stainless steel manufactured by selective laser melting (SLM). Describing Parameters must be defined and applied on the microstructure of these materials in their initial state and after loads were applied. The findings of this work form the basis for the investigation of AM material ageing.
Microbially influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) which act upon the metal by the reactiveness of hydrogen sulfide, and by withdrawal of the available electrons in electrical contact with the metal. Methanogenic archaea can also cause MIC by directly withdrawing electrons from the iron surface for methanogenesis. However, the mechanistic details and kinetics of the overall process are poorly understood. Precipitation of siderite, a by-product of methanogenesis, (4Fe + 5HCO3 + 5H+ 4FeCO3 + CH4 + 3H2O) can lead to an insulating layer on the metal surface and lower the corrosion rate. Still, the extent of FeCO3 precipitation may be significantly influenced by environmental conditions such as pH and advective processes.
To investigate early stage corrosion processes of stainless steel 1.4301 taking place during the biofilm formation of the organism Shewanella putrefaciens electrochemical impedance spectroscopy (EIS) in a multielectrode approach has been used. The multielectrode array consisted of up to 25 electrically isolated electrodes made of stainless steel wires of diameters ranging from 100 µm to 500 µm. They were connected to a multichannel microelectrode analyzer (MMA) electrically coupled through zero resistance ammeters. Current flow between electrodes in the array as well as changes in impedance of individual electrodes over time were recorded and analyzed with respect to the onset of localized corrosion and biofilm formation. The results were complemented by optical microscopy, SEM and AFM images which were taken immediately after the respective experiment. To verify that the multielectrode arrays correctly indicated the initial stages of the corrosion process and of biofilm formation they were introduced in a flow cell reaction vessel containing test specimens made from stainless steel 1.4301, which were checked regularly for signs of localized corrosion and biofilms. Preceding results with the multielectrode array in solutions containing high amounts of chloride ions and hydrogen peroxide at low pH also showed that it is possible with the MMA to monitor individual electrodes becoming local anodes as local corrosion set in, while the remaining electrodes predominantly acted as cathodes.
The governing load bearing mechanism of multi-pile foundations is often the shaft friction. Under cyclic loading the soil particles next to the foundation rearrange and tend to compact leading to a decrease of the surrounding normal stress. The reduction of the normal stress leads to a lower threshold for shear stress (friction fatigue), which results in a degraded shaft bearing capacity. The common interface models used for numerical simulations (e.g. Mohr-Coulomb) are not able to capture such behavior. This work aims to develop an interface material model that incorporates such features of the contact behavior at the soil-structure interface.
Combining CO2 Streams from Different Emitters – A Challenge For Transport And Storage Infrastructure
(2015)
The European Directive 2009/31/EC on the geological storage of CO2 envisages an open access of CO2 streams from different emitters to a nation- or even EUwide CO2 pipeline network if CO2 stream compositions meet “reasonable minimum composition thresholds”. As of today it is not known how such “composition thresholds” may be defined and which impurity levels may be viable in practical application.
To set up recommendations for criteria and respective threshold values for CO2 stream compositions, the project “CLUSTER” will investigate how a dynamic interplay – both in terms of mass fluxes and compositions – of CO2 streams from regionally clustered CO2 sources sharing a transport and storage infrastructure will impact corrosion, e.g., of pipelines and plant components, and geochemical alteration of cap rocks and reservoir rocks. In addition, the behaviour of such a highly dynamic CCS system will be considered for an overall optimization of system design including CO2 stream mixing schemes and facilities or interim CO2 storage.
In context of CLUSTER project, impacts of impurities (SO2, NO2, O2, CO, H2S, H2, N2, Ar and H2O) in CO2 streams captured from different sources in a regional cluster on transport, injection and storage were investigated. Corrosion studies of oxidizing, reductive or mixed atmospheres towards transport pipeline steel X70 were carried out applying high pressure (10 MPa) at low temperatures (278 K or 313 K).
We present the synthesis of four mesoporous templated iron oxides: Ferrihydrite, Hematite, Maghemite, Magnetite/Maghemite and the influence of water on the crystallization mechanism and the kinetics. The absence of water stabilize the ferrihydrite structure. By monitoring the dissolution in situ by using a QCMB and ex situ microscopy we got details in the dissolution mechanism of ferrihydrite.
Polynuclear aluminium species (Al13 keggin cluster) find application in different areas like water purification [1], contaminant transport [2], and as pilling clays with high specific surface areas[3], due to their strong binding ability to aggregates and high positive charge.
In the present contribution, we report on the in situ investigation of the Al13 sulfate synthesis by synchrotron wide-angle X-ray scattering (WAXS). Al13 cluster were crystallized by precipitating hydrolyzed aluminum solutions by the addition of sodium sulfate. The measurements were performed using a custom-made acoustic levitator as sample holder. The study provides information about the intermediates during the crystallization process. From the data, a mechanism was derived indicating the influence of the crystallization process.
Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. The exploration of the chemistry of metal phosphonates has gained considerable interest during the last decades due to their structural diversity. We synthesized manganese phosphonates in milling reactions. The mechanochemical reactions were investigated in situ to reveal the underlying mechanisms.
The exploration of metal phosphonates chemistry has gained great interest during the last decades, because of their structural diversity. Transition metal phosphonates are promising candidates for an application as electrocatalysts in oxygen evolution reactions (OER).
Here, we present the in situ investigation of mechanochemical syntheses of different manganese phosphonates by synchrotron X-ray diffraction. Nitrilotri(methylenephosphonic acid) and N,N-Bis(phosphonomethyl)glycine were chosen as ligands. The liquid-assisted milling process can be divided into three steps, including an amorphous stage. One of the products has not been obtained by classical solution chemistry before.
These metal phosphonates and/or their derivatives are considered to be active in electrochemical energy conversion. The verification of their applicability is one of the topics of our resent research.
Mechanochemistry is known for short reaction times, nearly quantitative conversions, and decreasing amount of solvents. Among organic syntheses, the Knoevenagel condensation is an important C-C bond forming reaction. We investigated the reaction of benzaldehyde derivates (nitro- and fluoro-derivates) with malononitrile syntheses by a combination of different in situ investigation techniques.
Mechanochemistry is a versatile approach for green and fast synthesis of pure substances. By milling the reactants, various organic, inorganic, and metal-organic compounds can be obtained in high yields. Although mechanochemistry is widely used, the underlying mechanisms are not fully understood making mechanochemical reactions difficult to predict. Metal phosphonates are metal-organic compounds accessible by grinding. Because of their structural diversity, the exploration of the chemistry of metal phosphonates has gained considerable interest during the last decades. Transition metal phosphonates are promising candidates for an application as electrocatalysts in oxygen evolution reaction (OER). Here, we present the in situ investigation of the mechanochemical synthesis of a manganese(II)-phosphonate by synchrotron X-ray diffraction and thermography. The product has not been obtained by classical solution chemistry before and its crystal structure was determined from PXRD data. The milling process can be divided into different steps, with the product crystallization corresponding with the highest temperature rise. The activity of this metal phosphonate towards OER was measured and is presented here.
In this contribution we describe an in-situ study of the crystallization of simvastatin in three solvents. The studies were carried out by solvent evaporation at the µSpot beamline using acoustically levitated solution droplets in combination with simultaneous X-ray diffraction, Raman spectroscopy, and imaging analysis.
Metal organic frameworks and coordination polymers play an important role in different fields of applications. Moreover, particularly fluorinated metal-organic frameworks (FMOFs) are in the focus of interest during the last years. In most cases, fluorine is implemented using perfluorinated organic linkers at the synthesis, usually performed by solvothermal synthesis. However, only few examples are known so far where fluorine is coordinated directly to the metal cation. Recently, we reported about mechanochemical syntheses and characterization of fluorine-containing coordination polymers of alkaline earth metals by milling M(OH) (M: Ca, Sr, Ba) with fluorinated benzene dicarboxylic acids 2 and we reported about mechanochemical syntheses of alkaline earth metal fluorides with ammonium fluoride. Now we are reporting about a combination of both synthesis routes. That is the first mechanochemical synthesis of coordination polymers where fluorine is coordinated directly to the metal cation.
In order to provide further evidence of damage mechanisms predicted by the solid-state transformation creep (SSTC) model, direct observation of damage accumulation during creep of Al–3.85Mg was made using synchrotron X-ray refraction (SXRR). X-ray refraction techniques capture the specific surface (i.e. surface per unit volume) with a field of view comparable to the specimen size but with microscopic sensitivity. A significant rise of the internal specific surface with increasing creep time was observed, providing evidence for the creation of a fine grain substructure, as predicted by the SSTC model.
Among the very few techniques to localize hydrogen (H) at the microscale in steels, Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a reliable tool. The necessity to detect hydrogen stems from its deleterious effects in metals, that are often used as structural components and to obtain better understanding of the underlying metallurgical mechanisms of hydrogen embrittlement (HE) which are still unclear.
Austenitic stainless steels are nowadays commonly used in a wide variety of application, from hydrogen transport and storage facilities to petrochemical and offshore applications where they are exposed to aggressive environments and therefore prone to HE. One of the greater risks in the austenitic class is the embrittlement of the material due to the instability of the γ austenite and its transformation into a brittle α martensitic phase. This transformation takes place due to the local stresses that are induced by the uptake of hydrogen during service. Nonetheless, it was shown that this transformation can occur as an artefact during SIMS analysis itself where Cs-sputtering is necessary not only to remove surface contaminations but mainly to enhance H/D secondary ion yield.
In the following contribution we show the influence of different sputtering conditions on AISI 304L austenitic stainless steel in order to distinguish the artefact from the hydrogen induced transformation. The material was charged electrochemically in a deuterium based electrolyte. Deuterium (D) must be in these experiments as a replacement for hydrogen which cannot be used because adsorbed hydrogen superimposes hydrogen originating from charging the sample in the SIMS images. ToF-SIMS analyses were conducted by ToF SIMS IV (IONTOF GmbH, Münster, Germany). The experiments were carried out on deuterium charged and non-charged samples. The structural characterization was carried out by SEM and EBSD examinations before and after charging, both with a Leo Gemeni 1530VP field-emission scanning electron microscope and a Zeiss Supra 40 instrument (Carl Zeiss Microscopy GmbH, Oberkochen, Germany). The results showed that the use of 1keV Cs+ beam induces stacking faults while higher sputter beam energies results in γ→α transformation.
Background Bacterial biofilms are regarded as the most common cause of chronic infections and are often associated with medical devices, such as implants and catheters. Bacteria growing in biofilms produce a protective, extracellular matrix, which enables them to tolerate much higher antimicrobial concentrations than free-living bacteria and survive long enough to acquire antimicrobial resistance. Preventive and therapeutic strategies against biofilm infections in clinical settings commonly involve the application of multiple antimicrobials: biocidal coatings on the biomaterials and systemically administered antibiotics. This frequent practice harbors the risk of the development of cross-resistance via shared resistance mechanisms between antimicrobials used in material coatings and administered antibiotics.
Aim Our goal is to determine how bacteria adapt to antimicrobials during biofilm formation on surfaces coated with antimicrobials and how population dynamics within biofilms affect the transmission of resistance mutations. Specifically, we want to identify antimicrobial-antibiotic-combinations that select for and against antibiotic resistance in biofilms by following the population dynamics of resistant and susceptible strains in competition assays on a single cell level.
Methodology To study the effect of antimicrobial-antibiotic exposure on resistance development and population dynamics on bacterial biofilms in a multidrug environment, we will grow Pseudomonas aeruginosa on glass surfaces with and without antimicrobial coatings and expose them to antibiotics. First, we will screen in vitro for combinations of antibiotics and antimicrobials that select for and against antibiotic resistance. Second, effective combinations will be chosen for in-depth investigations during bacterial adhesion and of mature biofilms of resistant and susceptible genotypes. Third, based on the outcome of the screen and the obtained mechanistic understanding we will choose a clinical example in which we study the relevance of our findings in biofilms grown in vivo.
Relevance Studying the biointerfacial interactions between bacterial biofilms and medical devices in terms of population dynamics as well as on single cell level during multidrug selection will help us understand how drug resistance develops and spreads in persistent biofilm infections. Based on our findings we aim to provide clinical recommendations for improved administration of antibiotics/antimicrobials in combination with medical device materials in order to mitigate against biofilm associated antimicrobial resistance.
Die Rasterkraftmikroskopie (AFM) hat sich in den letzten Jahren als eine vielseitige Abbildungstechnik von Oberflächen mit einer sehr hohen Ortsauflösung etabliert. Über die Untersuchung der reinen Oberflächentopographie sind erweiterte Modi in der Lage, gleichzeitig Informationen über die elektrischen und magnetischen Eigenschaften sowie Adhäsionsprozesse auf Oberflächen zu liefern. Interessanter wird es, wenn das AFM mit geeigneten Messzellen für in-situ-Untersuchungen in kontrollierten Atmosphären oder in Elektrolyten unter elektrochemischer Kontrolle ausgestattet ist. Dies ermöglicht die Untersuchung von Korrosions- und Adhäsionsprozessen unter Bedingungen, die die Betriebsumgebung repräsentieren.
Ein aktueller Forschungsschwerpunkt unseres Fachbereiches liegt in den Untersuchungen der Deformationseigenschaften von Funktionsschichten auf Leichtmetalllegierungen, sowie in situ Untersuchungen des Korrosionsverhaltens unter kombinierter korrosiver und mechanischer Beanspruchung mittels AFM. Durch die Integrierung eines Zug-Druckmoduls in den Probentisch des Rasterkraftmikroskops haben wir jetzt die Möglichkeit, verschiedene Materialien uniaxialen Umformversuchen mit bis zu 5 kN Kraft zu unterziehen. Dabei können unter anderem auch zyklische Belastungen genutzt werden, um Ermüdungsprozesse zu simulieren. Da die Messungen in situ ohne die De- und Remontage der Probe durchgeführt werden, ermöglicht der Aufbau nicht nur Messungen mit präziser Positionssteuerung, sondern auch die Untersuchung von Prozessen im elastischen Bereich, die für die Aufklärung der Mechanismen, die zu Ermüdungsversagen führen, entscheidend sind.
Die Posterpräsentation wird detaillierte Informationen zum neuen AFM-Setup liefern und unsere aktuellen Ergebnisse zur Verformung dünner Schutzschichten auf AA2024-T3 zusammenfassen.
THz and mid IR spectroscopy of high-molecular PE (HMW) and ultra high-molecular PE (UHMW) reveals modifications of the molecular structure. Characteristic absorption bands are changed if the two materials are exposed by -Co60 radiation up to 600 kGy and subsequently stored at an annealing temperature of 398 K until for 729 days. UHMW-PE and HMW-PE behave differently during the ageing process because of their molecular weight and inherent structure distinctions. The spectroscopic data offer characteristic absorption bands, which have been used to describe the complete ageing process in more detail. For instance, the integral absorption in the B1u THz-region can be used to describe quantitatively the reduction of crystallinity. The formation of trans vinylene unsaturation and the decay of vinyl during ageing can be observed in detail in the mid IR range.
Biomaterials for bone replacement and grafting should possess sufficient strength, be bioresorbable and demonstrate osteoconductivity/osteoinductivity. Nowadays, hydroxyapatite (HA) and tricalcium phosphate (TCP) are the most widespread ceramics for bone grafting at the market, however, their resorption is reported, in some cases, to be not enough. This is why the search for more soluble ceramics compared to HA and TCP looks rather viable.
A possible way to increase ceramics solubility leads to partial substitution of Ca2+-ions in Ca3(PO4)2 by alkali castions, like Na+ or/and K+. Improvement of solubility stems from decreasing lattice energy of a substituted phase, as well as increase in hydration energy of the ions releasing from the phase to ambient solution. From this viewpoint, bioceramics based on compositions from Ca3(PO4)2 - CaKPO4 - CaNaPO4 ternary system seems to be prospective for bone replacement and grafting in sense of resorption properties. At the same time, one should bear in mind that solubility level (resorbability) is governed not only by reduction of lattice energy, but also by microstructure features. Grain sizes and porosity contribute much to dissolution rate making study of sintering of aforementioned ceramics highly important.
Background Bacterial biofilms are regarded as the most common cause of chronic infections and are often associated with medical devices, such as implants and catheters. Bacteria growing in biofilms produce a protective, extracellular matrix, which enables them to tolerate much higher antimicrobial concentrations than free-living bacteria and survive long enough to acquire antimicrobial resistance. Preventive and therapeutic strategies against biofilm infections in clinical settings commonly involve the application of multiple antimicrobials: biocidal coatings on the biomaterials and systemically administered antibiotics. This frequent practice harbors the risk of the development of cross-resistance via shared resistance mechanisms between antimicrobials used in material coatings and administered antibiotics.
Aim Our goal is to determine how bacteria adapt to antimicrobials during biofilm formation on surfaces coated with antimicrobials, how antimicrobial resistance mutations are acquired and evolve within mature biofilms, and how population dynamics within biofilms affect the transmission of resistance mutations. Specifically, we want to identify antimicrobial-antibiotic-combinations that select for and against antibiotic resistance in biofilms by following the population dynamics of resistant and susceptible strains in competition assays.
Methodology We will grow biofilms of Pseudomonas aeruginosa on glass surfaces with and without antimicrobial coatings and expose them to antibiotics. Then we will track their physiological properties, evolutionary adaptations, and population dynamics. First, we will screen in vitro for combinations of antibiotics and antimicrobials that select for and against antibiotic resistance. Second, effective combinations will be chosen for in-depth investigations during bacterial adhesion and of mature biofilms of resistant and susceptible genotypes. Third, based on the outcome of the screen and the obtained mechanistic understanding we will choose a clinical example in which we study the relevance of our findings in biofilms grown in vivo.
Relevance Studying the biointerfacial interactions between bacterial biofilms and medical devices in terms of population dynamics as well as on single cell level during multidrug selection will help us understand how drug resistance develops and spreads in persistent biofilm infections. Based on our findings we aim to provide clinical recommendations for improved administration of antibiotics/antimicrobials in combination with medical device materials in order to mitigate against biofilm associated antimicrobial resistance.
Microbially influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) which act upon the metal by the reactiveness of hydrogen sulfide, and by withdrawal of the available electrons in electrical contact with the metal. Methanogenic archaea are supposed to cause MIC. Because they do not produce hydrogen sulfide, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood. Precipitation of siderite (4Fe + 5HCO3 + 5H+ 4FeCO3 + CH4 + 3H2O) can lead to an insulating layer on the metal surface and lower the corrosion rate. Still, the extent of FeCO3 precipitation may be significantly influenced by environmental conditions such as pH and advective processes.
Microbially influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) which act upon the metal by the reactiveness of hydrogen sulfide, and by withdrawal of the available electrons in electrical contact with the metal. Methanogenic archaea are supposed to cause MIC. Because they do not produce hydrogen sulfide, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood. Precipitation of siderite (4Fe + 5HCO3 + 5H+ 4FeCO3 + CH4 + 3H2O) can lead to an insulating layer on the metal surface and lower the corrosion rate. Still, the extent of FeCO3 precipitation may be significantly influenced by environmental conditions such as pH and advective processes.
Mechanochemistry is widely applicable for the synthesis of inorganic, metal-organic, and organic compounds. It is known for short reaction times, nearly quantitative conversions, and decreasing amount of solvents, which opens the field to more environmentally friendly syntheses routes. Among organic syntheses, the Knoevenagel condensation is an important C-C bond forming reaction leading to α,β-unsaturated compounds. To gain more information on the underlying processes, we investigated the syntheses by a combination of different in situ investigation techniques, including synchrotron X-ray diffraction, Raman spectroscopy and thermography. This combination provides information on the structural changes and temperature influences during milling. Benzaldehyde derivates (nitro- and fluoro-derivates) reacted with malononitrile to the respective benzylidenemalononitriles. The in situ investigations show direct and quantitative conversions. In the case of the fluorinated benzaldehyde derivates we showed the possibility of using liquid substrates in mechanochemical organic synthesis. Surprisingly, after crystallization from a viscous state, the material was suitable for single-crystal X-ray analysis.
The fundamental impact of sulfur and water on corrosion rates and potential failure of the exposed material is well known. However, the access to the related corrosion mechanism causing material degradation is often a problem to solve. This study investigates the effect of SO2 and water vapor in the initial stages of corrosion of an Fe9Cr0.5Mn model alloy at 650 °C in situ. The analysis was carried out under laboratory conditions using energy-dispersive X-ray diffraction (EDXRD).
The influence of heat treatment and creep loading on the microstructure of an Al-Cu-Li alloy was investigated. Especially the formation of different precipitates (T1 and Theta') were characterized and the microstructural changes under different ageing conditions (with and without external strain) were investigated to determine the effect od stress on the ageing process.
The duplex stainless steel 1.4062 (X2CrNiN22-2) is used as alternative material to austenitic stainless steels in the construction industry. The corrosion resistance of welded seams is influenced by the base material, the weld filler material, the welding process and also by the final surface treatment. The scale layer next to the weld seam can be removed by grinding, pickling, electro-polishing or blasting depending on the requested corrosion resistance. Blasted surfaces are often used in the industrial practice due to the faster and cheaper manufacturing process compared to pickled or electro-polished surfaces. Furthermore blasting with corundum-grain is more effective than blasting with glass-beads which also lower the process costs. In recent years, stainless steel surfaces showed an unusually high susceptibility to pitting corrosion after grinding with corundum. For this reason, it is now also questioned critically whether the corrosion resistance is influenced by the applied blasting agent. This question was specifically investigated by comparing grinded, pickled, corundum-grain- and glass-bead-blasted welding seams. Results of the SEM analyses of the blasting agents and the blasted surfaces will be presented and correlated with the results of different corrosion tests (KorroPad-testing and pitting potentials).
Due to their excellent combination of ductility, strength and corrosive resistance, austenitic stainless steels (ASS) are widely used in many industrial applications. Thus, these steel grades can be found as structural components in the (petro-)chemical industry, in offshore applications and more recent for storage and transport of hydrogen fuel. Steels employed for these applications are exposed to aggressive environments and hydrogen containing media. The ingress and accumulation of hydrogen into the microstructure is commonly observed during service leading to a phenomenon called “hydrogen embrittlement”. A loss in ductility and strength, the formation of cracks and phase transformations are typical features of this hydrogen-induced degradation of mechanical properties.
Although, great efforts are made to understanding hydrogen embrittlement, there is an ongoing debate of the underlying mechanisms. This knowledge is crucial for the safe use and durability of components on the one side and the development of new materials on the other.
Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was proven to be a powerful tool for depicting the distribution of the hydrogen isotope deuterium in the microstructure of austenitic and duplex steels. The combination with imaging techniques such as electron backscatter diffraction (EBSD) and scanning electron microscopy (SEM), delivering structural and morphological information, creates a comprehensive picture of the hydrogen/deuterium-induced effects in the materials. All the gathered data is treated with principal component analysis (PCA) and data fusion to enhance the depth of information.
The mobility of hydrogen and deuterium in a steel microstructure is affected by external mechanical stress. To investigate the behaviour of deuterium in a strained microstructure, a new in situ experimental approach was developed. This gives the possibility of analysing samples in the SIMS instrument simultaneously to four-point-bending-tests.
Specimens made from ASS AISI 304L were electrochemically charged with deuterium instead of hydrogen. This necessity stems from the difficulty to separate between artificially charged hydrogen and hydrogen existing in the pristine material or adsorbed from the rest gas in the analysis chamber. Nonetheless, similar diffusion, permeation and solubility data allow to draw qualitative conclusions from the experiments, which are relevant for the application addressed.
During the last years, there has been a rapid rise in the use of nanomaterials in consumer products. Especially silver nanoparticles are frequently used because of their well-known optical and antimicrobial properties. However, the toxicological studies focusing on silver nanoparticles are controversial, either claiming or denying a specific nano-efffect. To contribute to localizing nanoparticles in toxicological studies and to investigate the interaction of particles with cells, a fluorescent marker is often used to monitor their transport and possible degradation. A major problem, in this context is the issue of binding stability of a fluorescent marker which is attached to the particle.
In order to overcome this problem we provide an investigation of the binding properties of fluorescence-labeled BSA to small silver nanoparticles. Therefore, we synthesized small silver nanoparticles which are stabilized by poly(acrylic acid). The particles are available as reference candidate material and were thoroughly characterized in an earlier study. The ligand was exchanged by fluorescence marked albumin (BSA-FITC). The adsorption of the ligands was monitored by dynamic light scattering (DLS). To verify that the observed effects on the hydrodynamic radius originate from the successful ligand exchange and not from agglomeration or aggregation we used small angle X-ray scattering (SAXS). The fluorescent particles were characterized by UV/Vis and fluorescence spectroscopy. Afterwards, desorption of the ligand BSA-FITC was monitored by fluorescence spectroscopy and the uptake of particles in different in vitro models was studied.
The particles are spherical and show no sign of aggregation after successful ligand exchange. The fluorescence intensity is quenched significantly by the presence of the silver cores as expected, but the remaining fluorescence intensity was high enough to use these particles in biological investigations. Half-life of fluorescence labeling on the particle was 21 d in a highly concentrated solution of non-labeled BSA. Thus, a very high dilution and long incubation times are needed to remove BSA-FITC from the particles. Finally, the fluorescence-labeled silver nanoparticles were used for uptake studies in human liver and intestinal cells, showing a high uptake for HepG2 liver cells and almost no uptake in differentiated intestinal Caco-2 cells. In conclusion, we showed production of fluorescence-marked silver nanoparticles. The fluorescence marker is strongly adsorbed to the silver surface which is crucial for future investigations in biological matrices. This is necessary for a successful investigation of the toxicological potential of silver nanoparticles.
Microbiologically influenced corrosion (MIC) is the deterioration of metals due to the metabolic activities of microorganisms. Microorganisms can take electrons directly from the metal surface (EMIC) thereby causing corrosion. Well known culprits of EMIC are: sulfate-reducing bacteria (SRB), acetogens and methanogens.
Our aims
- Develop a novel flow system to study MIC by methanogens to mimic industrial Environments
- Investigate the inhibitory concentrations of biocides targeting SRB on corrosive methanogenic strains
- Investigate the inhibitory effects of corrosion inhibitors on methanogens
- Compare the inhibitory concentrations to SRB
Residual stresses are crucial when assessing the performance of welded components. The present work deals with the possibilities of transferring the real-life boundary conditions of welding, which influence the residual stress, into the laboratory. The possibilities of a test system specifically developed for this purpose with a maximum load capacity of 2 MN are shown. Due to the structural design, global process, geometry and material-dependent stresses are induced, which can be simulated and quantified within the system. Additionally, X-ray diffraction can be applied to determine the resulting local residual stress distribution precisely with high spatial resolution. Examples are presented how the conditions to be found during production are simulated in the laboratory. It is shown how welding residual stresses in high-strength steels are affected by the heat control. It was possible to clarify why elevated working temperatures significantly increase the tensile residual stresses in the heat affected zone (HAZ). The effect of a heat treatment applied under mechanical stress resulting from welding is demonstrated by the example of a creep resistant steel. Reheat cracking is significantly increased in this case compared to small scale laboratory based tests.
Hardness and pitting corrosion resistance are the major quality criteria of cutlery. Both are achieved by the heat treatment (austenitization, quenching and tempering) of the normally used martensitic stainless steels. The established quality control method regarding the pitting corrosion resistance is an alternating immersion test in 1 % NaCl solution at 60 °C according to DIN EN ISO 8442. This standard test shows a high deviation, which limits any optimization of the heat treatment process. New approaches for corrosion testing of martensitic stainless-steels were developed and used in the last years to connect the weak pitting corrosion resistance of martensitic stainless-steels with the phenomenon of chromium depletion. The tempering temperatures used in the industrial heat treatment of cutlery are too low to explain the appearance of chromium depletion. For this reason, a systematic investigation of three heat treatment parameters (austenitization time, cooling speed and tempering temperature) were performed on the martensitic stainless-steels X50CrMoV15 (1.4116) to detect their contribution to chromium depletion. The electrochemical potentiodynamic reactivation (EPR), which is very sensitive to any change of the microstructure, was used to quantify the degree of chromium depletion. The KorroPad indicator-test was applied to correlate low pitting corrosion resistance to the presence of chromium depletion. The results of all investigations allow conclusions about the very small process window, which is necessary to achieve cutlery with high pitting corrosion resistance.
The KorroPad indicator test was invented at the Federal Institute for Materials Research and Testing to detect stainless-steel surfaces susceptible to pitting corrosion. The KorroPad indicator test is thus an interesting alternative for manufacturers, processors, users and researchers to time consuming exposition experiments and complex electrochemical investigations, which are normally used to reveal surface-related processing errors resulting in reduced pitting corrosion resistance. Furthermore, the KorroPad indicator test can be used to visualize alloy- and microstructure-related factors causing susceptibility to pitting corrosion. The detection limit of the KorroPad indicator test was characterized in this work using reference alloys with different chromium content (5 % to 18 %). The alloy-specific detection limit was shifted successfully to higher chromium content by increasing the concentrations of NaCl and K3[Fe(CN)6]. The modified KorroPads can now be used to establish an alloy-specific quality control regarding the pitting corrosion resistance of different stainless steel grades.
In Vorbereitung einer Restaurierung erfolgten naturwissenschaftliche Untersuchungen zu Schadensphänomenen und Glaszusammensetzungen an mittelalterlichen Gläsern aus der Dorfkirche in Koszewko (Polen)im Environmental Scanning Electron Microscope (ESEM) mit EDX. Die Ergebnisse zeigen, dass die Glasverwitterung schon sehr stark vorangeschritten ist und ein zukünftiger Schutz der mittelalterlichen Glasmalereifelder vor Umwelteinflüssen unbedingt notwendig ist. Es wurde ein Schutzverglasungsystem entwickelt, das speziell auf den langfristigen Erhalt der einzelnen mittelalterlichen Glasmalereifelder ausgelegt ist.
Nickel-free, nitrogen alloyed austenitic stainless-steels, with about 19 wt.-% Mn and 0,8 wt. % N, are an interesting alternative to classic CrNi austenitic stainless steels due to their superior mechanical properties (Rm > 900 MPa, A5 > 50 %, Av > 350 J) in the solution annealed condition. The formation of chromium-rich nitrides during suboptimal heat treatment, processing or application leads to an inhomogeneous distribution of alloying elements in the microstructure, which reduces the corrosion resistance. Consequently, an accurate knowledge of the sensitization behavior is indispensable for the use of nickel-free, high-nitrogen austenitic stainless steels. The relationship between artificial aging, phase formation and corrosion resistance was investigated on the alloys X8CrMnN18-19 (1.3815) and X8CrMnMoN18-19-2 (1.4456), both alloyed with 0,8 wt.-% Nitrogen, in the present work. The microstructural evolution was studied by LM and SEM while the corrosion resistance was characterized with the electrochemical potentiodynamic reactivation (EPR) and the KorroPad indicator-test. Both alloys showed increased corrosion susceptibility within critical aging parameters. Finally, a sensitization diagram was described successfully for both alloys showing the positive effect of molybdenum.
The copper alloyed stainless steel 1.4542 (X5CrNiCuNb16-4) is used in different areas due to its good mechanical properties and corrosion resistance. Strength and corrosion re-sistance can be adjusted by the heat treatment, which is of importance for the application of this alloy. The mechanical properties (strength and hardness) are attributed to the dispersive precipitation of the copper rich ε–Phase. The additional precipitation of chromium carbides can reduce the corrosion resistance. Different ageing states were produced to investigate the precipitation behaviour with various methods. Furthermore, the influence of cold-rolling on the precipitation behaviour was studied in comparison to a solution annealed state without deformation. The microstructure was studied by SEM and the variations of hardness and magnetic proportion were characterised. The electrochemical potentiodynamic reactivation (EPR) was used to determine the corrosion resistance and detect chromium depletion in all heat-treated states. The results show that a work hardening accelerates the precipitation rate, while ageing at 600 °C reduces the corrosion re-sistance due to chromium depletion.
A numerical pre-study has shown that cracks in a flat sample featuring a drilled hole can be classified into one of three crack shape classes based on the combined evaluation of various types of test data.
Tanks for heating oil made of polyethylene grades have been on the market since the early 1970s in Germany. Tank manufacturers recommend the replacement of the tanks after a period of 30 years due to guarantee safety. Polyethylene grades are subject to ageing by alteration of the properties during their life cycle. The degree of ageing and the nature of the degradation process mainly depend on the chemical degradation of the polyethylene, the wall thickness of the tank and the environmental conditions. There are no results available on the long-term behavior of the polyethylene grades, especially after a service life of more than 30 years. The aim of this investigation was the determination of the factual degree of damage in comparison to the uncontaminated polyethylene grades. Material data of the used polyethylene grades are available because the BAM was the competent authority for the tests and expert reports for the approval of these tanks until the middle of the 1990s.
The determination of the Melt Flow Rate (MFR) and the Fourier Transmission IR Spectroscopy (FTIR) of tank sections from the bottom, the shell and the roof of 10 segregated heating oil storage tanks produced of polyethylene grades A and B were used as tests methods.
The MFR measurements of the tank sections showed differences in the values depending on the weight which was used (5 kg or 21.6 kg). A reduction of the MFR values was measured for most of the sections of tanks made of polyethylene grade B after a service life of the tanks of more than 30 years. This grade is mainly subject to the internal ageing by cross-linkages, increased degree of branched molecules and loss of the plasticizer, and to a lesser extent by oxidative degradation. The FTIR analysis, especially of tank sections of the bottom and the shell showed that the intensity of the CH2 asymmetric and symmetric stretching vibrations in the range: 2800 - 2900 cm-1 and the CH2 bending deformation vibration at 1400 cm-1 increased due chain scissions. The intensity of the carbonyl stretching vibration C=O at 1740 cm-1 is low. The carbonyl index characterizes the degree of oxidation.
Microbiologically influence corrosion (MIC) has become a big concern due the increased usage of different metals by our society. Microorganisms can use metal as an electron donor, causing unpredictable but serious damages. Nowadays it is known that besides sulfate reducing bacteria (SRB), other microorganisms including acetogens, iron oxidizers and methanogens can also induce MIC. Current studies related to methanogen-induced MIC (MI-MIC) mainly focused on environmental isolates from the oil and gas industry (e.g. Methanococcus maripaludis) with industrial materials e.g. iron. However, MI-MIC can occur in many other environments as well, including the oral cavity. Methanobrevibacter oralis is a methanogen isolated from the human oral cavity and was found more frequently in patients suffering from peri-implantitis/periodontitis. Titanium-implants removed from those patients have also showed clear signs of corrosion. The aim of our study is to establish and analyze corrosion potentials of dental metals (e.g. titanium) by oral methanogens. Periodontal pockets samples from patients suffering from periodontitis/peri-implantitis were taken for methanogenic and SRB enrichments. Stainless steel, pure titanium or Ti-6Al-4V alloy was used for corrosion studies. Corrosion rates and methane production were measured using weight-loss method and gas chromatography, respectively. Metal surfaces were visualized with scanning electron microscopy. Microbial communities in the dental pockets of healthy people and patients will be compared using 16S rRNA amplicon sequencing. Overall, this is the first study investigating the susceptibility of different dental implant materials to corrosion using human-related Archaea. The outcomes of this study can be further explored for a variety of clinical applications.
Additive manufacturing (AM) offers an effective solution to the medical sector. It enables the production, on demand, of customised implants which match the patient’s anatomy, with grafts that promote bone growth, as well as surgical guides that help the surgeons.
The objective of this project is to provide a comprehensive basis to enable the safe use of medical AM products with traceable and reliable dimensionalmeasurements. This will guarantee the reliability of medical AM products to notified bodies and facilitate acceptance of AM in the medical sector for a better quality of life.
Collective Orientational Order and Phase Behavior of a Discotic Liquid Crystal under Confinement
(2018)
Discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to self-organize into columns in a hexagonal columnar mesophase, driven by the overlapping of the π orbitals of their aromatic cores. This leads to a high charge-carrier mobility along the column axis. Embedding liquid crystals into nanopores of anodic aluminum oxide (AAO) results in a 2D nanoconfinement of these materials. This confinement affects their properties, compared to the bulk, such as phase transition temperatures and enthalpies, molecular mobility, and crystallization.
In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6) was confined into parallel aligned cylindrical nanopores of AAO membranes by melt infiltration. The membrane as confining hosts used have varying pore diameters, from 10 nm to 160 nm, covering a broad pore size range, thus, a better understanding of the confinement effect on phase behavior and molecular configuration in the pores. Furthermore, it is aimed to obtain axial ordering or to increase degree of axial ordering by chemically modifying the surfaces of the pores. Therefore, the pore surfaces the membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. The phase behavior was explored by a power-compensated DSC allowing the detecting of small changes in the phase behavior. In the literature, dielectric spectroscopy was demonstrated as a method to monitor molecular order inside the pores. Here, we also investigate the collective orientational order, corresponding to dominating molecular ordering, by dielectric spectroscopy.
Over the past decades research on the molecular dynamics of miscible polymer blends are of topical interest in the literature, in an attempt to understand the segmental mobilty of individual components, as it is affected by blending. In general, miscible polymer blends exhibit a complex behavior of the molecular mobility. For an A/B blend the relaxation times of component A and component B are affected by the spatial local compositional heterogeneity, present in binary systems on a microscopic level, regardless of the macroscopic homogeneity. Here, a combination of broadband dielectric and specific heat spectroscopy was employed to study the dynamically asymmetric PVME/PS blend with seven different compositions, focusing on samples with high PS contents. Considering that PS is dielectrically invisible, BDS is a powerful technique to study the response of PVME, as it is affected by PS segments. In this work the well-known binary relaxation times distribution of PVME in a blend, originating from the spatial local heterogeneity, was studied over ten decades in frequency, for the first time in literature. Secondly, one of the detected processes, α’-relaxation, shows a crossover from high-temperature behavior (system in equilibrium) towards a low temperature regime, where PS undergoes the thermal glass transition, resulting in confined segmental dynamics of PVME within a frozen network of PS. Here, we introduce a precise mathematical tool to distinguish between the temperature dependency regimes of the process, and examine the composition dependence of the crossover temperature, detected by dielectric spectroscopy. Moreover, the dielectric data was compared in detail with results obtained by specific heat spectroscopy. This comparison provides new insights in the dynamics and dynamic heterogeneity of the PVME/PS blend system.
Since discovery of discotic liquid crystals (DLCs), consisting of a disklike rigid aromatic core and flexible alkyl chains attached to the core, dating back to Chandrasekhar’s work in 1977, they have been extensively investigated to reveal their fundamental properties and potential for applications. The researches on DLCs in last decades showed that DLCs can be considered as promising materials for organic electronic applications since they exhibit one dimensional high charge mobility along the column axis in a columnar mesophase. The mobilies of the rigid aromatic core and the flexible alkyl chains can influence their application properites, e.g. the charge carrier mobility, therefore, it needs to be explored in detailed.
In this study, a series of dipole functionalized triphenylene-based discotics, forming a columnar mesophase, were investigated to reveal the influence of the functionalization on phase behavior, molecular dynamics and as well as conductivity. The molecular mobility of the discotics was probed by broadband dielectric spectroscopy (BDS). In addition to conductivity and localized dynamics, glassy dynamics were also observed. The phase behavior of the material was explored by a power-compansated differential scanning calorimetry (DSC). Beside the phase transition temperatures and enthalpies, thermal glass transitions were found for all the materials. Moreover, the glassy dynamics were further investigated by Flash DSC, which is a chip-based calorimetry technique allows fast heating and cooling rates as high as 10000K/s.
Dynamics of nanoscopically confined PVME in thin films of an asymmetric miscible PVME/PS blend
(2018)
In recent years, substantial efforts have been devoted to investigating nanoscopic confinement of polymers, and its effect on glassy dynamics. Broadband Dielectric Spectroscopy (BDS) was used to study the dynamics of ultra-thin films of PVME/PS 50/50 wt% blend, employing a novel nano-structured capacitor sample arrangement. The investigated system shows a complex dynamic behavior. First, an α-relaxation, related to a bulk-like layer was found. Second, an α’-relaxation was observed, characteristic for dynamically asymmetric blends, where the out of equilibrium dynamics is attributed to weakly-cooperative PVME segments relaxing within a frozen environment of PS segments. Third, for thinnest films, an Arrhenius-like process was dominant in the dielectric spectra, indicating localized fluctuations of the segments. Relaxation rates of this process resembled that of the degenerated α-relaxation of the adsorbed layer, found for pure PVME [1], thus it was assigned accordingly. For thinnest films, this process undergoes a further confinement, due to the topological constraints, introduced by PS. Such multiple confinement effect has not been reported for ultra-thin films of polymer blends, before this study [2].
[1] Madkour, S. et al. ACS Appl. Mater. Interfaces 2017, 9, 7535.
[2] Madkour, S. et al. ACS Appl. Mater. Interfaces 2017, 9, 37289.
Effective hydrogen storage capacities are prerequisite for an efficient energy provision using fuel cells. Since glass has low intrinsic hydrogen permeability, it is a promising material for hydrogen storage containers as well as hydrogen diffusion barriers. Previous studies on oxidic glasses suggest a correlation between the glass composition and hydrogen permeation that was derived mainly from silica glass. In the present study, we concentrate on the relationship between thermodynamic (i.e., configurational entropy) and topologic (i.e., free volume, network polymerization) parameters. Experimental data were gathered well below the glass transition temperature, excluding significant effects caused by structural relaxation and chemical dissolution of hydrogen. The results of seven analysed glasses on the SiO2-NaAlO2 joint showed that the hydrogen permeability in fully polymerized glasses cannot solely be derived from the total free volume of the glass structure. Hence, evidence is provided that the size distribution of free volume contributes to hydrogen solubility and diffusion. Additionally, the results indicate that the configurational heat capacity ΔCp at Tg affects the hydrogen permeability of the investigated glasses.
- UCNPs were succesfully synthesized and characterized
- Various stages of UCNP growth were tracked using different
analytical methods including real time in-situ & time-resolved
luminescence spectroscopy, SAXS and TEM measurements
- Additional size determination will be performed using inductively
coupled plasma - mass spectrometry (ICP-MS)
We demonstrate a 2D platform based on high contrast wetting patterns suitable for miniaturized microbiological assays.
In principal, superhydrophilic spots are surrounded by a superhydrophobic surface area. The special structure of the superhydrophilic functional surface ensures that liquids, e.g. bacterial suspensions or biocide solutions, spread immediately and evenly on this surface without passing the wetting boundary. This feature allows a homogenous distribution of bacteria or chemical substances on well defined lateral dimensions. The superhydrophilic spots may also serve as substrate for bacterial biofilms. Due to the high wetting contrast and the fabrication process, it is possible to minimize the test areas as well as their distance to each other.
We demonstrate the fabrication process of the high wetting contrast platform and also present a microbiological assay as an application example. Advantages of this platform are the use of low volumes and its potential of automated analysis.
Mit nicht-konformen oder schlecht dokumentierten Prüfergebnissen können weder Behörden noch Unternehmen etwas anfangen. Belastbare und eindeutige Informationen aus den Registrierungsdossiers sind entscheidend, damit industrielle und gewerbliche Verwender der Stoffe das Gefahrenpotenzial einschätzen und ggf. Maßnahmen zum Schutz von Menschen und Umwelt treffen können.
Darüber hinaus benötigen die Behörden verlässliche Daten aus den Registrierungen, um ihrer Verantwortung bei der Identifizierung regulierungsbedürftiger Stoffe nachkommen zu können.
The quenching and partitioning (Q&P) heat treatment enables a higher deformability of high strength martensitic steels. The Q&P heat treatment was applied on the martensitic stainless steel 1.4034 (X46Cr13) to study the influence of partitioning time. Therefore, extensive characterizations of the mechanical properties, focussing on the materials behaviour under different mechanical load scenarios, were performed. A comprehensive analysis of the microstructural evolution was per-formed for different heat treatment and mechanical loading states. A complete solution of chromium carbides was detected to be a first requirement for successful Q&P heat treatment. The comparison of common quenching and tempering with the Q&P heat treatment verifies the extensively enhanced materials strength whereat the formability is still acceptable. The microstructural reason was detected to be an increasing aus-tenite fraction due to austenite reversion at subgrain boundaries of martensite besides the stabilising of retained austenite. Further a distinctive strength differential effect was observed.
Microbially influenced corrosion (MIC) of iron is usually attributed to sulfate-reducing microorganisms (SRM) which act upon the metal by the reactiveness of hydrogen sulfide, and by withdrawal of the available electrons (Fe → Fe²⁺ + 2e⁻ ; E° = 0.47 V) in electrical contact through surface attachment. Also methanogenic archaea are supposed to cause MIC. Because they do not produce hydrogen sulfide, withdrawal of electrons may be their main corrosive mechanism; however, mechanistic details and kinetics of the overall process are poorly understood. Precipitation of siderite (4Fe + 5HCO₃⁻ + 5H⁺ → 4FeCO₃ + CH₄ + 3H₂O) can lead to an insulating layer on the metal surface and lower the corrosion rate. Still, the extent of FeCO₃ precipitation may be significantly influenced by environmental conditions such as pH and advective processes.
To investigate the corrosive potential of methanogens, we studied strains isolated from marine sediments (Methanococcus maripaludis 14266, 2067, Methanobacterium-affiliated strain IM1), crude oil tanks (Methanococcus maripaludis Mic1c10, KA1) and the oral cavity (Methanobrevibacter oralis) in a closed (batch) culture, and in a sand-packed flow-through cell with pH control and simulation of a fluctuating environment. Results indicate that the rates of iron corrosion due to coupled methanogenesis (up to 0.3 mm/yr) are comparable to that caused by SRM. Surface analyses of the metal showed severe pitting. Such knowledge and deeper understanding also from an electrokinetic point of view may not only provide further models in microbial electrophysiology, but also contribute to mitigation strategies in MIC.
Microbiologically influenced corrosion (MIC) is the deterioration of metals due to the metabolic activities of microorganisms. Microorganisms can take electrons directly from the metal surface (EMIC) thereby causing corrosion. Well known culprits of EMIC are: sulfate-reducing bacteria (SRB), acetogens and methanogens.
The presence of water in the surrounding atmosphere of a propagating crack has a major influence on the subcritical crack growth. While these external phenomena are well understood, there is still a lack of knowledge on the influence of structurally bound water on crack propagation. Thus, our recent study aims on the analysis of crack propagation in water bearing soda-lime silicate glasses with up to 8 wt.% water. The samples were synthesized in an internally heated pressure vessel at 0.5 GPa. Since this preparation route limits the sample sizes, standard test geometries allowing for the determination of stress intensity factors, such as double cantilever beam, are not feasible. Thus, radial cracks in the hydrous glasses were initiated by Vickers indentation and crack growth was simultaneously captured with a camera system. An automated image analysis algorithm was used for the analysis of the crack length of each single video frame. To minimize influences by atmospheric water, all experiments were conducted in a glovebox purged with dry N2. About 150 cracks per glass composition were analyzed to provide statistical significance of the Vickers-induced SCCG. The results show that structurally bound water has a major influence on SCCG by means of crack lengths, growth rates and time of crack initiation.
Statistical analysis of Vickers induced subcritical crack growth in soda-lime silicate glasses
(2018)
Studies on Vickers induced subcritical crack growth are controversially discussed since the stresses that drive the crack growth are distributed three dimensionally within the material and cannot be retraced by available methods. Hence, empirical approaches are used to calculate mechanical material parameters such as the stress intensity factor KI. However, the results of these approaches show large deviations from those measured by standardized techniques such as double cantilever beam (DCB) or double cleavage drilled compression (DCDC). Yet, small specimen sizes and low specimen quantities can prevent the execution of DCB and DCDC measurements. Here we present an approach that is based on a statistical analysis of Vickers induced radial cracks. For this purpose more than 150 single radial cracks were analyzed. The cracks were generated in a commercial soda-lime silicate glass. The experiments were performed in a glovebox purged with dry nitrogen gas to minimize the influence of atmospheric water on crack growth. The temporally resolved evolution of the radial cracks was monitored in-situ using an inverted microscope equipped with a camera system directly below the Vickers indenter. An automated image analysis software was used to determine the crack length over time. The data show that the crack propagation and thereby the crack velocities are not uniformly but statistically distributed. These findings allow, using the statistical mean value of the distributions in combination with DCB data, a precise formulation of KI for each measured crack length.
Premature failure of glass under load is caused by sub-critical crack growth (SCCG) originate from microscopic flaws at the surface. While SCCG is related to the humidity of the ambient atmosphere, leading to stress corrosion phenomena at the crack tip, the detailed mechanism and the effect of different network formers are still not fully understood. For more clarity, various soda silicate glasses with a second network former were investigated by double cantilever beam technique: Na2O*Al2O3*SiO2 (NAS), Na2O*B2O3*SiO2 (NBS), Na2O*PbO*SiO2 (NPbS).
Three effects on the crack growth velocity, v, versus stress intensity, KI, curves were found out. The slope in region I, which is limited by corrosion, increases in the order NAS < NBS ≲ NPbS. The velocity range of region II reflecting the transition between corrosion effected and inert crack growth (region III), varies within one order of magnitude between the glasses. The KI region of inert crack growth strongly scatters between 0.4 and 0.9 MPam1/2. For comparison, crack growth at different humidity in commercial soda lime silicate glass (NCS) was measured.
There is a need for an assessment of the emission properties of volatile organic compounds (VOCs) from consumer products. A method comparison was carried out to evaluate adapted and cost-effective procedures for such items. Smaller and automated emission chambers de-picted similar kinetics compared to a 203 L standard chamber. Toy samples made of PVC (Polyvinyl chloride) emitted more VOCs compared to other tested polymeric products. The emissions from 2 selected samples were studied to allow an evaluation of the resulting room concentration and external exposure of a child. Obtained concentrations were not of concern.
Comparison of Formaldehyde Concentrations in Emission Test Chambers Using EN 717-1 and EN 16516
(2018)
For many years EN 717-1 (Wood-based panels - Determination of formaldehyde release - Part 1: Formaldehyde emission by the chamber method) is the standard for formaldehyde emission testing of wooden boards. In 2017 EN 16516 (Construction products - Assessment of release of dangerous substances - Determination of emissions into indoor air) was published as a new harmonised standard for the emission testing of construction products. Because test chamber conditions are different, both standards give different concentrations for formaldehyde. For the determination of a conversion factor four test series were set up with different wooden boards.
The Ni-Cr-Mo-W alloy is characterized by the excellent high-temperature corrosion resistance, good strength and ability to work in aggressive environments. To protect the surface of the substrate 13CrMo4-5 steel against aggressive environments the Inconel 686 as clad layer was used. The corrosion process was performed in oxidizing mixture of gases like O2, COx, SOx. The second part of corrosion Experiment concerned the corrosion test of the coating in reducing atmosphere of the specified gases with ashes, which contained e.g. Na, Cl, Ca, Si, C, Fe, Al.
BAM ensures and represents high standards for safety in technology and chemistry. Additive manufacturing (AM) changes the requirements for conventional non-destructive testing (NDT) as new processes of defect creation occur. Especially in safety critical areas, such as aerospace and automotive, new manufacturing processes and materials always require reliability tests and new standards which is a big challenge for NDT.
The influence of isothermal ageing on microstructure, sensitisation and pitting corrosion resistance of the lean duplex stainless steel (LDSS) X2CrNiN23-4 was investigated with various electrochemical methods. The aging at 600 °C (from 0.1 h up to 20 h) lead to the formation of precipitations at the ferrite-ferrite (α/α) and ferrite-austenite (α/γ) grain boundaries, inducing sensitisation due to chromium depletion. The degree of sensitisation was evaluated with the double loop electrochemical potentiokinetic reactivation method (DL-EPR) according to ASTM G108 and correlated with critical pitting potentials (Epit) as well as critical pitting temperature (CPT) measured in an electrolyte according to ASTM G48 using electrochemical noise. Up to an ageing time of 1 h, the sensitisation did rise significantly, stabilising at a nearly constant level with a slight drop at 20 h. This behaviour correlated perfectly with the potentiodynamically determined pitting potentials Epit and sensitisation. The CPT showed a higher sensitivity at short ageing times compared to the DL-EPR and Epit. Finally, the KorroPad method was applied to visualise the sensitisation induced reduction of pitting corrosion resistance. The “KorroPad” is an agar-based gel-electrolyte containing 0.1 mol/l sodium chloride (NaCl) and 0.1 mol/l potassium ferricyanide III (K3[Fe(CN)6]), invented at the Federal Institute of Materials Research and Testing in Berlin (Germany) to detect surfaces of stainless steel prone to pitting corrosion. The standard configuration of the KorroPad showed no differentiation for the various aging conditions. Increasing the concentration of both NaCl and potassium ferrocyanide III to 0.5 M shifts the detection limit of the KorroPad method to stainless steels with higher corrosion resistance, producing the same trends detected by standard electrochemical pitting corrosion values (Epit, CPT) and sensitisation (DL-EPR). By that, the KorroPad method was successfully adjusted to the lean-duplex stainless steel X2CrNiN23-4, enabling short-time testing to detect sensitization.
Sintered bioactive glass scaffolds of defined shape and porosity, e.g. made via additive manufacturing, must provide sufficient bioactivity and sinterability. As higher bioactivity is often linked to high corrosion and crystallization tendency, a certain compromise between sintering ability and bioactivity is therefore required. Groh et al. developed a fluoride-containing bioactive glass (F3), which allows fiber drawing and shows a bioactivity well comparable to that of Bioglass®45S5.
To study whether and to what extent the sinterability of F3 glass powder is controlled by particle size, coarse and fine F3 glass powders (300-310µm and 0-32µm) were prepared by crushing, sieving and milling. Sintering, degassing and phase transformation during heating were studied with heating microscopy, vacuum hot extraction (VHE), DTA, XRD, and SEM.
For the coarse glass powder, sintering proceeds slowly and is limited by surface crystallization of primary Na2CaSi2O6 crystals. Although the crystallization onset of Na2CaSi2O6 is shifted to lower temperature, full densification is attained for the fine powder. This finding indicate that certain porosity might be tuned via particle size variation. Above 900°C, intensive foaming is evident for the fine powder. VHE studies revealed that carbon species are the main foaming source.
The importance of molecular conformation for polymorphism and its repercussions in terms of tight control over the industrial production of crystalline organic materials with highly reproducible physicochemical properties has long been recognized. Efforts to understand how a crystallization solvent can direct the formation of a polymorph containing a specific molecular conformation are, however, relatively scarce. Nicotinic acid (NA) and its hydroxyl derivatives (2-, 4-, 5-, and 6-hydroxynicotinic acids) are very good models for such studies. Indeed, regardless of the solvent, NA always crystallizes as a single polymorph with the molecule in the same neutral conformation. In contrast, the hydroxyl derivatives are prone to polymorphism and solvate formation and, depending on the crystallization conditions, the molecules in the crystal lattice can exhibit hydroxyl, oxo, or zwitterionic conformations. The present study focused on 5-hydroxynicotinicacid (5HNA) shows that by judicious selection of the solvent it is possible to obtain 1:1 solvates, where solvation memory is not completely lost and the tautomer preferred in solution persists in the crystalline state: zwitterionic in 5HNA·H2O and neutral in 5HNA·DMSO. Nevertheless, upon thermal desolvation the obtained materials evolve to the same unsolvated form where the molecule is in a zwitterionic conformation. The structures of 5HNA·H2O and 5HNA·DMSO obtained from single crystal-ray diffraction are discussed and compared with that of 5HNA solved from powder data. The energetics of the dehydration/desolvation process was also fully characterized by thermogravimetry (TG), differential scanning calorimetry (DSC) and Calvet microcalorimetry.
The Scaled Boundary Finite Element Method (SBFEM) is a semi-analytical method that shows promising results in modelling of guided ultrasonic waves. Efficiency and low computational cost of the method are achieved by a discretisation of the boundary of a computational domain only, whereas for the domain itself the analytical solution is used. By means of the SBFEM different types of defects, e.g. cracks, pores, delamination, corrosion, integrated into a structure consisting of anisotropic and isotropic materials can be modelled.
In this contribution, the SBFEM is used to analyse the propagation of guided waves in a structure consisting of an isotropic metal bonded to anisotropic carbon fibre reinforced material. The method allows appropriate wave types (modes) to be identified and to analyse their interaction with different defects. Results obtained are used to develop a structural health monitoring system for composite pressure vessels used in automotive and aerospace industries.
Sialic acid (SA) is a cell surface glycan, which has a strong role in many cell activities including differentiation, proliferation, and the immune response. The amount of SA has been found to be correlated with cancer, with an upregulation on more aggressive cancers. Therefore, there is great interest in developing methods for detection of SA on cancer cells. We are screening SA on cancer cell lines by using fluorescent molecularly imprinted polymers, SA-MIPs.Macrophages, which evolve from mono-cytes, are well known for their extraordinary ability to phagocytose foreign objects. This could lead to the hypothesis that the SA-MIPs can be recognized by macrophages as foreign object; thus leading to internalization and potential degradation. We have discovered that SA-MIPs can be detected after incubation with the RAW macrophage cells, with increasing fluorescence over time. The microscopy analysis shows that the RAW cells ingest the SA-MIP particles. This information is important when planning to use SA-MIPs in future in vivo applications.
Sialic acid (SA) is a cell surface glycan, which has a decisive role in many cell activities including differentiation, proliferation, and the immune response. The amount of SA has been found to correlate with cancer, with an upregulation on more aggressive cancers. Therefore, there is a great interest in developing methods for detection of SA on cancer cells. We are screening SA on cancer cell lines by using fluorescent molecularly imprinted polymers, SA-MIPs. Macrophages, which evolve from mono-cytes, are well known for their extraordinary ability to phagocytose foreign objects. This could lead to the hypothesis that the SA-MIPs can be recognized by macrophages as foreign object; thus leading to internalization and potentially degradation.
We have demonstrated that SA-MIPs can be detected after incubation with the RAW macrophage cells, with increasing fluorescence over time. The microscopy analysis shows that the RAW cells ingest the SA-MIP particles. This information is important when planning to use SA-MIPs in future in vivo applications.
Cancer is a leading cause of death worldwide, and its early detection and resultant treatment contributes significantly to patient recovery and survival. Detection is currently based on magnetic resonance imaging and computed tomography, methods that are expensive, while processing of the results is time consuming. There is a need for low-cost cancer-detection techniques that give conclusive results in the shortest time possible. Molecularly imprinted polymers (MIPs) targeting tumor markers on cancerous cells may provide a cheaper solution for cancer detection. Thin MIP layers immobilized on particle platforms are known to give faster response times and increased selectivity in comparison to bulk MIPs. It has been reported that a fluorescent monomer can be incorporated into the MIP layer, allowing for faster detection of the target group, thus significantly shortening the turn-around time for biopsies.
Changes in sialylation patterns of cell surface glycoproteins indicate malignancy. Here, we present the development of MIPs that target sialic acid-terminated glycoproteins (SA MIPs), prepared as a thin layer on a silica nanoparticle platform. A fluorescent monomer is incorporated into the MIP layer, and upon binding of the target group to the specific binding pockets in the MIP, the fluorescence signal is enhanced. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) are used for structural characterization. To validate the specificity, fluorescence changes of MIPs in the presence and absence of template are compared to their corresponding non-imprinted polymer particles (NIP). Initial binding experiments with tumor cells using fluorescence microscopy demonstrate that the presented technique shows promise as a cheaper alternative to current detection methods, while allowing for relatively shorter analysis of biopsy results.
Additive manufacturing (AM) offers a range of novel applications. However, the manufacturing process is complex and the production of defect-free parts with a high reliability is still a challenge. Thermography is a valuable tool for process surveillance, especially in metal AM processes. The high process temperatures allow one to use cameras usually operating in the visible spectral range. Here, we compare the results of first measurements during the manufacturing process of a commercial laser metal deposition (LMD) setup using a MWIR camera with those from a VIS high-speed camera with band pass filter in the NIR range.
Additive manufacturing (AM) opens the route to a range of novel applications.However, the complexity of the manufacturing process poses a challenge for the production of defect-free parts with a high reliability. Since process dynamics and resulting microstructures of AM parts are strongly influenced by the involved temperature fields, thermography is a valuable tool for process surveillance. The high process temperatures in metal AM processes allow one to use cameras usually operating in the visible spectral range to detect the thermally emitted radiation from the process. In our work, we compare the results of first measurements during the manufacturing processes of a commercial laser metal deposition (LMD) setup and a laser beam melting (LBM) setup using a MWIR camera with those from a VIS high-speed camera with band pass filter in the NIR range.